Methanol → HCID 178491826、化合物

HRID 2095650ノート

反応式

HRID 2095650 の反応式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([O:9][CH3:10])[C:3]=1[C@H:11]([C:13]1[C:21]2[C:16](=[N:17][CH:18]=[C:19]([C:22]3[C:23]([CH3:39])=[N:24][N:25]([C@H:28]4[CH2:33][CH2:32][C@H:31]([C:34]([O:36]CC)=[O:35])[CH2:30][CH2:29]4)[C:26]=3[CH3:27])[CH:20]=2)[NH:15][CH:14]=1)[CH3:12].CO.[OH-].[Li+].O>>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([O:9][CH3:10])[C:3]=1[C@H:11]([C:13]1[C:21]2[C:16](=[N:17][CH:18]=[C:19]([C:22]3[C:23]([CH3:39])=[N:24][N:25]([C@H:28]4[CH2:33][CH2:32][C@H:31]([C:34]([OH:36])=[O:35])[CH2:30][CH2:29]4)[C:26]=3[CH3:27])[CH:20]=2)[NH:15][CH:14]=1)[CH3:12]

参加物

5

反応物 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 178472400HCID 178472400、化合物

生成物 1

HCID 178491826HCID 178491826、化合物

実験手順

A solution of ethyl trans-4-(4-{3-[(1S)-1-(2-chloro-3-fluoro-6-methoxyphenyl)ethyl]-1H-pyrrolo[2,3-b]pyridin-5-yl}-3,5-dimethyl-1H-pyrazol-1-yl)cyclohexanecarboxylate (9.00 mg, 0.0163 mmol) in MeOH (1 mL, 30 mmol) was added lithium hydroxide (1.95 mg, 0.0814 mmol) and H2O (0.4 mL, 20 mmol). The mixture was stirred at rt for 2 h. The organic solvent was removed in vacuo, and the material was extracted with DCM and water at pH 2. The organic layer was concentrated in vacuo to afford the title compound as a white solid. MS (ES+): m/z=525.21/527.21 (100/50) [MH+]. HPLC: tR=1.45 min (polar—3 min, UPLC-ACQUITY).

後処理

  1. customThe organic solvent was removed in vacuo
  2. extractionthe material was extracted with DCM and water at pH 2
  3. concentrationThe organic layer was concentrated in vacuo

出典と根拠

ORDレコード
ord-70c2fcf4758941899aa191050bf3f82b
出典データセット
uspto-grants-2013_05
特許番号
US08445510B2

反応ノート

読み込み中…